CN114068286B - Photoionization source ion migration tube - Google Patents
Photoionization source ion migration tube Download PDFInfo
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- CN114068286B CN114068286B CN202111410919.4A CN202111410919A CN114068286B CN 114068286 B CN114068286 B CN 114068286B CN 202111410919 A CN202111410919 A CN 202111410919A CN 114068286 B CN114068286 B CN 114068286B
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- 230000005012 migration Effects 0.000 title claims abstract description 29
- 238000013508 migration Methods 0.000 title claims abstract description 29
- 150000002500 ions Chemical class 0.000 claims abstract description 103
- 238000001514 detection method Methods 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims description 43
- 238000004061 bleaching Methods 0.000 claims description 11
- 230000005684 electric field Effects 0.000 claims description 11
- 239000012212 insulator Substances 0.000 claims description 6
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 claims description 5
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims description 5
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 3
- 230000009471 action Effects 0.000 claims description 2
- 230000003287 optical effect Effects 0.000 claims description 2
- 230000002093 peripheral effect Effects 0.000 claims description 2
- 229910052594 sapphire Inorganic materials 0.000 claims description 2
- 239000010980 sapphire Substances 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 abstract description 11
- 238000005516 engineering process Methods 0.000 abstract description 9
- 238000001228 spectrum Methods 0.000 abstract description 9
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 238000001871 ion mobility spectroscopy Methods 0.000 description 10
- 229910052743 krypton Inorganic materials 0.000 description 9
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 description 9
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 6
- 239000008096 xylene Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 230000004323 axial length Effects 0.000 description 2
- -1 xylene ion Chemical class 0.000 description 2
- 231100000481 chemical toxicant Toxicity 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 description 1
- 230000037427 ion transport Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Abstract
The invention provides a photoionization source ion migration tube. The vacuum ultraviolet lamp is used as a light source, the beam expander system is arranged right in front of the vacuum ultraviolet lamp light window, the diameter of a light beam output by the vacuum ultraviolet lamp is enlarged by more than N times, the whole inner cavity of an ionization region of the ion transfer tube is filled with vacuum ultraviolet light, and the problems of low target sample utilization rate and low detection sensitivity caused by non-uniformity of ultraviolet light distribution in the ionization region and non-uniformity of sample distribution in the ion transfer spectrum of the traditional photoionization source are solved. The photoionization source ion transfer tube technology disclosed by the invention improves the utilization efficiency of target sample molecules in the ionization region to be close to 100%, so that high-number-density target sample product ions are obtained in the ionization region, and the detection sensitivity of the photoionization source ion transfer tube is improved. The migration tube is simple in design and strong in universality. The beam expander system can isolate the vacuum ultraviolet lamp from the gas phase of the target sample, so that the pollution of a light window is avoided, and the service life of the lamp is prolonged.
Description
Technical Field
The invention relates to an ion migration tube of a core component of an ion migration spectrometer, in particular to a photoionization source ion migration tube which adopts a beam expander system to expand the diameter of a light beam output by a vacuum ultraviolet lamp, improves the utilization rate of neutral sample molecules in an ionization region and further obtains high detection sensitivity.
Background
The atmospheric pressure photoionization technology is the most commonly used ionization technology in ion mobility spectrometry, and is widely applied to the detection fields of volatile organic pollutants, explosives, drugs, chemical toxicants and the like. Early photoionization techniques generally employed lasers as the light source, and were first introduced by Lubman et al in 1982 into the field of ion mobility spectrometry (Anal. Chem.1982, 54:1546). With the advent of miniaturized commercial vacuum ultraviolet lamps (VUV lamps), hill and Eiceman et al used Krypton VUV lamps and hydro VUV lamps directly as photoionization sources for ion mobility spectrometry (Anal.Chem.1983, 55:1761;Anal.Chem.1986,58:2142). In order to improve the detection sensitivity and the detection target range of the photoionization source ion mobility spectrometry, spangler in 1992 discloses a photoionization source ion mobility spectrometry technology of an axial side fixed structure, which adopts a Krypton VUV lamp as a photoionization source (US 5338931). Hans-Rudiger et al in 1997 disclose a Dopant doping-based high-sensitivity photoionization source ion mobility spectrometry technology (US 5968837) for detecting positive and negative targets by photoionization source ion mobility spectrometry. Li Haiyang et al in 2012 disclose an array type photoionization source ion transfer tube technique to enhance the detection sensitivity in the negative ion mode.
Commercial VUV lamps commonly used in photoionization source ion mobility spectrometry have a smaller beam diameter of only 8mm for outputting vacuum ultraviolet light. Ion mobility spectrometry to ensure good ion transport efficiency, the ionization region inner diameter is usually set to 12 to 24mm. This results in the presence of vacuum ultraviolet light only in the tiny columnar areas immediately adjacent to the axis within the ionization region, and no vacuum ultraviolet light in the radial areas slightly farther from the axis within the ionization region. Li Haiyang et al have recently studied the spatial distribution characteristics of the sample concentration in the ionization region and found that the sample gas does not form a uniform spatial distribution of the sample concentration after entering the ionization region, and that the sample gas of high concentration is mainly distributed in a radial region slightly off-axis inside the ionization region (Sensor act. B-chem.2022,350: 130844). The non-uniformity of ultraviolet light distribution and sample distribution in the ionization region causes that only a small part of samples in the ionization region can be photoelectronized to form product ions, the sample utilization rate is low, and the ion mobility spectrometry detection sensitivity is low.
Disclosure of Invention
The invention provides a photoionization source ion migration tube with high sensitivity. The photoelectric ionization source of the ion transfer tube adopts a vacuum ultraviolet lamp as a light source, a beam expander system is arranged right in front of a vacuum ultraviolet lamp light window, the diameter of a light beam output by the vacuum ultraviolet lamp is enlarged by more than N times, the whole internal cavity of an ionization region of the ion transfer tube is filled with vacuum ultraviolet light, and the problems of low target sample utilization rate and low detection sensitivity caused by non-uniformity of ultraviolet light distribution in the ionization region and non-uniformity of sample distribution in the ion transfer spectrum of the traditional photoionization source are solved. The photoionization source ion transfer tube technology disclosed by the invention can improve the utilization efficiency of target sample molecules in an ionization region to be close to 100%, and obtain high-number-density target sample product ions in the ionization region, so that the detection sensitivity of the photoionization source ion transfer tube is improved.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
The ion transfer tube is a hollow cylindrical cavity formed by alternately and coaxially overlapping an annular electrode and an annular insulator from left to right, wherein the left end of the cavity is provided with a photoionization source, the right end of the cavity is provided with an ion receiving electrode, an ion gate is arranged between the photoionization source and the ion receiving electrode along the direction from the photoionization source to the ion receiving electrode, the interior of the cavity is divided into two areas, an ionization area is formed between the photoionization source and the ion gate, and a transfer area is formed between the ion gate and the ion receiving electrode;
The photoionization source comprises an ionization source chamber, a vacuum ultraviolet lamp, a light input lens and a light output lens;
The ionization source chamber is a cylindrical barrel with a sealed left end and an open right end, the right open end of the barrel is in sealing connection (or sealed connection) with the left end face of the annular electrode at the left end of the ionization region through an annular insulator, a through hole is formed in the left end face of the inside of the barrel along the axial direction, a vacuum ultraviolet lamp is arranged in the through hole, and the light output direction of the vacuum ultraviolet lamp points to the inside of the barrel along the axis of the barrel;
Two light input lenses and light output lenses which are mutually spaced and arranged in parallel are arranged in the ionization source chamber from left to right, the axes of the cylindrical light input lenses and the cylindrical light output lenses coincide with the axis of the ionization source chamber, the peripheral edges of the cylinders of the light input lenses and the cylindrical light output lenses are in airtight connection with the inner wall surface of the ionization source chamber, the light input lenses are positioned between the vacuum ultraviolet lamp and the light output lenses, and the light input lenses and the light output lenses form a beam expander system;
The vacuum ultraviolet lamp outputs a cylindrical parallel beam with the diameter of d 1, the cylindrical parallel beam is converted into a cylindrical parallel beam with the diameter of d 2 after passing through the beam expander system and is input into an ionization region, the diameter d 2 is larger than the diameter d 1, the inside (radial and axial regions of the inside) of the ionization region is filled with vacuum ultraviolet light, and neutral sample molecules entering the ionization region are ionized by the vacuum ultraviolet light to form sample product ions;
The left end face of the light input lens is a concave spherical surface, the symmetry axis of the concave spherical surface is coaxial with the light input lens, the right end face of the light input lens is a plane, the plane is perpendicular to the axis of the light input lens, the left end face of the light output lens is a plane, the plane is perpendicular to the axis of the light output lens, the right end face of the light output lens is a convex spherical surface, the symmetry axis of the convex spherical surface is coaxial with the light input lens, the optical focal points of the light input lens and the light output lens are overlapped, and the focal length f 2 of the light output lens is larger than the focal length f 1 of the light input lens;
The ultraviolet light output by the vacuum ultraviolet lamp has any one wavelength or the mixture of more than two wavelengths including 147.6nm, 130.0nm, 129.0nm, 123.9nm, 121.6nm and 116.9 nm;
The light input lens and the light output lens are made of the same material, and the material is any one of sapphire, magnesium fluoride and lithium fluoride;
a sample gas inlet is formed in the circumferential side wall, close to the ion gate, of the ionization region, an air outlet is formed in the circumferential side wall, close to the photoionization source, of the ionization region, and a drift gas inlet is formed in the ion receiving electrode;
Setting an axial nonuniform direct current electric field with an ion enrichment function in an ionization region, gradually weakening the electric field strength along the direction from an ion source to an ion receiving electrode, and setting an axial uniform direct current electric field in a migration region;
One path of sample gas enters an ionization region through a sample gas inlet, is ionized by vacuum ultraviolet light output by a photoionization source to form product ions, and the product ions migrate to a region of the ionization region, which is close to an ion gate, under the action of a non-uniform direct current electric field in the ionization region and are enriched;
The product ions in the ionization region are injected into the migration region in a pulse ion group mode by the ion gate which is opened for a short time period, are sequentially driven by a uniform direct current electric field to reach the ion detection electrode to realize separation and detection, and are converted into two-dimensional spectrogram information of current intensity versus time to be output;
One path of bleaching gas enters the interior of the migration zone through a bleaching gas inlet and flows out of the migration zone along the direction opposite to the ion flight direction, and finally flows out of the ion migration tube through an air outlet together with the gas in the ionization zone;
The gas of the bleaching gas is any gas or a mixture of more than two gases including gases such as O 2、N2、CO2、H2 and Ar.
The invention has the advantages that:
The photoionization source ion transfer tube technology disclosed by the invention can improve the utilization efficiency of target sample molecules in the ionization region to be close to 100%, so that target sample product ions with high number density are obtained in the ionization region, and the detection sensitivity of the photoionization source ion transfer tube is further improved. The migration tube is simple in design and strong in universality. In addition, the use of the beam expander system can isolate the vacuum ultraviolet lamp from the gas phase of the target sample, thereby avoiding the pollution of a light window and prolonging the service life of the lamp. The invention is described in further detail below with reference to the accompanying drawings:
Drawings
FIG. 1 is a schematic view of a photoionization source ion transfer tube employing the disclosed technique.
Wherein: 1. a photoionization source; 2. an ionization region; 3. an ion gate; 4. a migration zone; 5. an ion receiving electrode; 6. a ring electrode; 7. a ring-shaped insulator; 8. a bleaching gas inlet; 9. a sample gas inlet; 10. a tail gas outlet; 11. an ionization source chamber; 12. a Krypton VUV lamp; 13. shan Aomian light input lenses; 14. shan Tumian light output lenses. Shan Aomian the light input lens 13 and Shan Tumian the light output lens 14 are both made of magnesium fluoride.
FIG. 2 is a schematic view of the structure of the ion transfer tube of the photoionization source without using the beam expander system. Wherein: 1. a photoionization source; 2. an ionization region; 3. an ion gate; 4. a migration zone; 5. an ion receiving electrode; 6. a ring electrode; 7. a ring-shaped insulator; 8. a bleaching gas inlet; 9. a sample gas inlet; 10. a tail gas outlet; 11. an ionization source chamber; 12. a Krypton VUV lamp; 13. a biplane lens; 14. a biplane lens. The biplane lens 13 and the biplane lens 14 are made of magnesium fluoride.
FIG. 3 (a) an ion mobility spectrum obtained for a 1ppm xylene sample in a photoionization source ion mobility tube (e.g., FIG. 1) as disclosed herein; (b) Ion mobility spectra of 1ppm xylene samples were obtained in a photoionization source ion mobility tube (as in fig. 2) without the use of a beam expander system.
Detailed Description
Example 1
The structure of the photoionization source ion migration tube adopting the technology disclosed by the invention is shown in figure 1.
The photoionization source 1 adopts a Krypton VUV lamp 12 with photon energy of 10.6eV as a vacuum ultraviolet light source, the Krypton VUV lamp 12 is fixed at the left end of a metal cylindrical ionization source chamber 11 with the outer diameter of 30mm and the inner diameter of 18mm, a Shan Aomian light input lens 13 and a Shan Tumian light output lens 14 with the outer diameter of 18mm are sequentially arranged in the ionization source chamber 11 along the light output direction of the Krypton VUV lamp 12, the Shan Aomian light input lens 13 and the Shan Tumian light output lens 14 are made of magnesium fluoride, and the Shan Aomian light input lens 13 and the Shan Tumian light output lens 14 form a beam expander system, so that the diameter of a Krypton VUV lamp output beam is expanded from 8mm to 18mm.
The ion gate 3 is a Bradbury-Nielsen type ion gate, and is formed by weaving metal wires with the diameter of 0.05mm on a tetrafluoroPCB polar plate, the wire spacing is 0.3mm, and the metal wires on the ion gate are divided into two groups which are mutually insulated and are respectively connected with two pulse high-voltage power supplies; the ion receiving electrode 5 is a faraday disk with a diameter of 6mm and is fixed on a metal shielding cylinder with an outer diameter of 30 mm.
The ionization region 2 and the migration region 4 are formed by alternately overlapping annular conductive pole pieces 6 with axial lengths of 5mm, inner diameters of 18mm and outer diameters of 30mm and annular insulating pole pieces 7 with axial lengths of 5mm, inner diameters of 18mm and outer diameters of 30mm, the length of the ionization region 2 is 30mm, the length of the migration region 4 is 75mm, and an axial uniform direct current electric field of 800V/cm is arranged in the ionization region 2 and the migration region 4.
The temperature of the ion transfer tube is 110 ℃, zero air with 500mL/min of bleaching gas enters the ion transfer tube through a bleaching gas inlet 10, the sample gas is zero air containing 1ppm of dimethylbenzene, the flow rate is 100mL/min, the sample gas enters an ionization region 2 of the ion transfer tube through a sample gas inlet 11, and the bleaching gas and the sample gas finally flow out of the ion transfer tube through a tail gas outlet 12.
FIG. 3a shows an ion mobility spectrum of a 1ppm xylene sample obtained from the operation of the photoionization source ion mobility tube disclosed in the present invention under the above experimental conditions. Wherein the migration time of the xylene ion spectrum peak is 2.84ms, and the current intensity of the xylene ion spectrum peak is 556pA.
Comparative example 1
In order to compare and show the performance of the photoionization source ion transfer tube technology disclosed by the invention in terms of improving the sample utilization rate and further improving the sample detection sensitivity, in the experimental process, the uniconcave light input lens 13 and Shan Tumian light output lens 14 inside the photoionization source 1 in the photoionization source ion transfer tube shown in fig. 1 are replaced by a double-plane lens 13 and a double-plane lens 14 with the outer diameter of 18mm, so that the photoionization source ion transfer tube without using a beam expander system is formed, as shown in fig. 2. The structure and other operating parameters of the ion transfer tube remain unchanged.
Since the biplane lens 13 and the biplane lens 14 can only keep the Krypton VUV lamp output beam passing through without damage, the beam cannot be expanded, and the ion spectrum peak intensity of the 1ppm xylene sample is only 275pA, as shown in fig. 3 b. The peak intensity of the ion spectrum is reduced by half compared to fig. 3 a.
Claims (7)
1. The utility model provides a photoionization source ion migration tube, the ion migration tube is annular electrode (6) and annular insulator (7) from left to right coaxial coincide constitution's cavity in proper order, set up photoionization source (1) in the cavity left end, the right-hand member sets up ion receiving pole (5), along photoionization source (1) to ion receiving pole (5) orientation, set up ion gate (3) in the cavity inside between photoionization source (1) and ion receiving pole (5), divide into two regions with the cavity inside, wherein constitute ionization region (2) between photoionization source (1) and ion gate (3), constitute migration region (4) between ion gate (3) and ion receiving pole (5), its characterized in that:
The photoionization source (1) comprises an ionization source chamber (11), a vacuum ultraviolet lamp (12), a light input lens (13) and a light output lens (14);
the ionization source chamber (11) is a cylindrical barrel with a closed left end and an open right end, the right open end of the barrel is in sealing connection or airtight connection with the left end face of the annular electrode (6) at the left end of the ionization region (2) through the annular insulator (7), a through hole is formed in the left end face of the barrel along the axial direction, a vacuum ultraviolet lamp (12) is arranged in the through hole, and the light output direction of the vacuum ultraviolet lamp (12) points to the inside of the barrel along the axis of the barrel;
Two light input lenses (13) and light output lenses (14) which are mutually spaced and arranged in parallel are arranged in the ionization source chamber (11) from left to right, the axes of the cylindrical light input lenses (13) and the cylindrical light output lenses (14) are overlapped with the axis of the ionization source chamber (11), the peripheral edges of the cylinders of the light input lenses (13) and the cylindrical light output lenses (14) are in airtight connection with the inner wall surface of the ionization source chamber (11), the light input lenses (13) are positioned between the vacuum ultraviolet lamp (12) and the light output lenses (14), and the light input lenses (13) and the light output lenses (14) form a beam expander system;
The vacuum ultraviolet lamp (12) outputs a cylindrical parallel beam with the diameter of d 1, the cylindrical parallel beam is converted into a cylindrical parallel beam with the diameter of d 2 after passing through the beam expander system and is input into the ionization region (2), the diameter d 2 is larger than the diameter d 1, the inside (radial and axial regions inside) of the ionization region (2) is filled with vacuum ultraviolet light, and neutral sample molecules entering the ionization region (2) are ionized by the vacuum ultraviolet light to form sample product ions;
the light input lens (13) and the light output lens (14) are made of the same material, and the material is any one of sapphire, magnesium fluoride and lithium fluoride.
2. The photoionization source ion transfer tube of claim 1, wherein:
the left end face of the light input lens (13) is a concave spherical surface, the symmetry axis of the concave spherical surface is coaxial with the light input lens (13), the right end face of the light input lens (13) is a plane, the plane is perpendicular to the axis of the light input lens (13), the left end face of the light output lens (14) is a plane, the plane is perpendicular to the axis of the light output lens (14), the right end face of the light output lens (14) is a convex spherical surface, the symmetry axis of the convex spherical surface is coaxial with the light input lens (14), the optical focal points of the light input lens (13) and the light output lens (14) are overlapped, and the focal length f 2 of the light output lens (14) is larger than the focal length f 1 of the light input lens (13).
3. The photoionization source ion transfer tube of claim 1, wherein:
The ultraviolet light (12) outputs ultraviolet light with any one wavelength or the mixture of more than two wavelengths including 147.6nm, 130.0nm, 129.0nm, 123.9nm, 121.6nm and 116.9 nm.
4. The photoionization source ion transfer tube of claim 1, wherein:
Sample gas inlets (9) are formed in the circumferential side walls, close to the ion gate (3), of the ionization region (2), gas outlets (10) are formed in the circumferential side walls, close to the photoionization source (1), of the ionization region (2), and drift gas inlets (8) are formed in the ion receiving electrode (5).
5. The photoionization source ion transfer tube of claim 1, wherein:
an axial nonuniform direct current electric field with an ion enrichment function is arranged in the ionization region (2), the electric field intensity is gradually weakened along the direction from the ion source (1) to the ion receiving electrode (5), and an axial uniform direct current electric field is arranged in the migration region (4).
6. The photoionization source ion transfer tube of any one of claims 1 to 5, wherein:
One path of sample gas enters the ionization region (2) through the sample gas inlet (9), is ionized by vacuum ultraviolet light output by the photoionization source (1) to form product ions, and the product ions migrate to the region of the ionization region (2) close to the ion gate (3) under the action of a non-uniform direct current electric field in the ionization region (2) and are enriched;
The product ions in the ionization region (2) are injected into the migration region (4) in a pulse ion group mode by the ion gate (3) which is opened for a short time period, are driven by a uniform direct current electric field to reach the ion detection electrode (5) in sequence to realize separation and detection, and are converted into two-dimensional spectrogram information of current intensity versus time to be output;
One path of the bleaching gas enters the migration zone (4) through the bleaching gas inlet (8) and flows out of the migration zone (4) along the direction opposite to the ion flight direction, and finally flows out of the ion migration tube together with the gas in the ionization zone (2) through the gas outlet (10).
7. The photoionization source ion transfer tube of claim 6, wherein: the gas of the bleaching gas is any gas or a mixture of more than two gases including O 2、N2、CO2、H2 and Ar gas.
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|---|---|---|---|
| CN202111410919.4A CN114068286B (en) | 2021-11-25 | Photoionization source ion migration tube |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111410919.4A CN114068286B (en) | 2021-11-25 | Photoionization source ion migration tube |
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| CN114068286A CN114068286A (en) | 2022-02-18 |
| CN114068286B true CN114068286B (en) | 2024-07-16 |
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| CN216849840U (en) * | 2021-11-25 | 2022-06-28 | 中国科学院大连化学物理研究所 | Photoionization source ion migration tube |
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| CN216849840U (en) * | 2021-11-25 | 2022-06-28 | 中国科学院大连化学物理研究所 | Photoionization source ion migration tube |
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